Apparatus for the distillation and fractionation of composite liquids and control means therefor



July 19, 1949.

| B. BRAGG ET AL APPARATUS FOR THE DISTILLATION AND FRACTIONATION OF COMPOSITE LIQUIDS AND CONTROL MEANS THEREFOR Original Filed April 22, 1941 CONTROL SYSTEM.

' 5 Sheets-Sheet l ATTORNEY ET AL L, B. BRAGG Hb DISTILLJATION AND FRACTIONATION QUIDS AND CONTRO L MEANS THEREFOR July 19, 1949.

' APPARATUS FOR T COMPOSITE LI Original Filed April 22, 1941 5 Sheets-Sheet 2 INVENTORS [ESL/E 5. E466 (HWARZLE/E BY (UTHEERT J. B/eow/v. 5

ATT

QIUQQQU NW Noh MGM, awn, mum.

MQN OWN XVNAQUNRW v 3 2 lllllllll i! WOW VOW NMN July 19, 1949. D BRAGG -j- 2,476,280

APPARATUS FOR THE DISTILLATION AND FRACTIONATION OF COMPOSITE LIQUIDS AND CONTROL MEANS THEREFOR Original Filed April 22, 1941 5 Sheets-Sheet 3 INVENTORS LESLIE B. BRAGG (Mai: A .Scmmez; ER

' 5 Sheets-Sheet 4 AND FRACTIONATION OF OL MEANS THEREFOR L. B BRAGG ET AL APPARATUS FOR THE DISTILLATION COMPOSITE LIQUIDS AND CONTR ed. April 22, 1941 Original Fil INVENTORS LEISUE B -5'A AGG (HA/e455 A. SCHWARZLER BY Cur/vaaerf Beowxv.

ATTORNEY 2,476,280 N OF IIii: B. BRAGG ET AL Jufiy 19, W49.

APPARATUS FOR T DISTILLATION AND FRACTIONATIO COMPOSITE LIQUIDS AND CONTROL MEANS THEREFOR Original Filed April 22, 1941 5 Sheets-Sheet 5 NWM WwM

MOM

NTOR BPAGG HWAEZLEIQ BERT INVE A554 x4" 8 66448455 A 5:

. hhm mvm \M Wm OWN VIWM II 'I Patented July 19, 1949 UNITED STATES PATENT OFFICE APPARATUS FOR THE DISTILLATION AND FRACTIONATION OF COMPOSITE LIQUIDS AND CONTROL MEANS THEREFOR Leslie B. Bragg, Scotch Plains, N. J and Charles A. Schwarzler and Cuthbert J. Brown, Foxboro, Mass., assignors to Foster Wheeler Corporation, New York, N. Y., a corporation of New York Continuation of application Serial No. 389,756, April 22, 1941. This application May 10, 1944,

Serial No. 534,974

10 Claims.

the vapors leaving the still will be rich in the lightest boiling constituents of the charge at the beginning of the distillation operation, and will become poorer in the lighter constituents and richer in the heavier constituents of the charge as the distillation progresses. With an efiicient fractionating column, when distillation begins, the vapors at the top of the column will consist of the lightest boiling constituents of the charge in an almost pure state, and as the distillation progresses, the lightest constituents will be removed from the charge in the still, and eventually a transition point will be reached at which the light constituents are substantially all removed, and the temperature at the top of the column will rise quickly to the boiling temperature of the next heavier constituent.

With batch distillation apparatus employing a condenser at the top of the column which totally condenses the vapors leaving the column, and

with the condensate returned to distributing means at the top of the column, it is possible to remove the overhead products stream from the distributing means b a pump through a cooler and a flow recorder controller. By regulating the rate of removal of the overhead stream through the pump, and with a fixed rate of heat input and constant rate of vaporization in the still, it is possible to regulate the reflux ratio within the fractionating column at will. The first product removed will be almost pure product having a boiling point substantially that of the pure lightest constituents in the charge. As distillation continues and the lightest constituents in the charge become less concentrated in the charge, the temperature at the top of the column will tend to rise slowly due to the fact that the column is not capable of completely removing from the vapors all of the higher boiling material. During the early stages of distillation, when the vapors from the still are rich in the lightest boiling constituent, a comparatively low ratio of liquid returned to the column to product withdrawn from the column, or a comparatively low reflux ratio, is sufiicient to produce an overhead product of the desired purity. How ever, as vapors leaving the still become less concentrated in the lightest boiling constituents, it becomes necessary to increase the reflux ratio in order to maintain the desired degree of purity. Whatever the reflux ratio may be, as the distillation progresses the overhead product eventually will become impure to the extent that the temperature at the top of the column will tend to rise above the boiling temperature of the product of specified desired purity. In consequence, it is possible to assign a series of temperatures in the vapor stream at the top of the column or in the stream flowing from the column, which may be utilized as control indications and control temperatures for varying the reflux ratio as desired. One method of accomplishing this is by regulation of the valves in the product lines connected with the tower.

Accordingly, the invention provides a method of, and apparatus for, batch distillation of composite fluids, which utilizes the temperature at the top of a fractionating column or the temperature in the vapor stream flowing from the top of the column, as a basis for the automatic regulation of the reflux ratio in the column and for the automatic operation of the valves controlling the lines through which products flow from the column. By utilizing this method and apparatus, products of the desired degree of purity may be obtained automatically, and with a considerably smaller consumption of heat than would be required for the production of prod ucts of similar purity by previously practiced methods of operation which utilize a fixed minimum reflux ratio, or a variable reflux ratio manually controlled. The automatic control also includes automatic means for shutting down the distillation unit at the end of the batch distillation run, and in the event of high still pressure, low steam pressure, power failure or air failure, and for automatically restarting the unit.

The invention will be understood from the following descrlption when considered in connection with the accompanying drawings forming a part thereof and in which:

Fig. 1 is an elevational View, showing more or less diagrammatically, one form of apparatus embodying, and for carrying out, the invention;

Fig. 2 is a view similar to Fig. 1 but in greater detail, showing part of the control system;

Fig. 3 shows more or less diagrammatically, another part of the control system;

Fig. 4 is a diagrammatic view of the Wheatstone bridge arrangement of the control system;

Fig. 5 is a diagrammatic view of a detail of the control system, and

Fig. 6 is a diagrammatic view of a part of the pressure-temperature compensating device utilized in the control system.

Like characters of reference refer to the same or to similar parts throughout the several views.

Referring to the drawings, particularly to Fig. 1 thereof, reference character designates a shell still to which heat is supplied by means of a steam coil |3 within the still, and steam issupplied to this coil through a line H. Condensate of the steam is withdrawn from the coil through line into a trap l6 and is withdrawn from the trap through line H. The vapors evolved in the still are conducted through a transfer line H! to the lower part of a fractionating column I9 having vapor and liquid contact apparatus 25 therein positioned above the outlet of the transfer line l8. Any suitable type of vapor and liquid contact apparatus ma be utilized. In this instance, the column has packing of the type shown in Stedman United States Patent No. 2,047,444, granted July 14, 1936. Vapors leave the fractionating tower |9 through a vapor line 2| and are totally condensed in a shell and tube type of surface condenser 22 into which cooling fluid is introduced through line 23 and is withdrawn through line 24. Condensate of the vapors is returned to the top of the tower through a line 2| and is collected on a condensate collectin device 25 of any suitable form, which functions also to distribute the condensate substantially uniformly over the packing '20. A portion of the condensate collecting on the device 25 is withdrawn through a line 26 by one of pumps 21, which force it through line 28 into a product cooler 29, and the cooled condensate is delivered to line 30 from which it is withdrawn through any one of product lines 3|, 32, 33, 34, 35, 36, 31 or 38, depending upon which portion of the feed stock is being condensed in the condenser 22 at the time. For simplicity in illustration, but three product lines are shown in Fi Reflux is returned to the still (Fig. 2) through line 40 which connects with line 4|! and line 42' which is controlled by a slop valve 42 which is by-passed by a valve controlled line 43. Line 40 also is provided with a flow indicator 44. Line 40' connects through line 4| with line 45 through which residue is withdrawn from the still. Liquid in line 38 which is to be returned to the feed tank flows through line 45 which connects with charge line 41. Line 46 is controlled by a slop valve 48 which is lay-passed by a valve controlled line 49. The still is charged through line 41, pump 50, lines 5|, 4|), 4| and 45. Residue is withdrawn from the still through lines 45 and 4|, pump 50, line 52, cooler 53 and line 54. The lines 40, 40', 4|, 42', 45, 46, 41, 5| and 52 are controlled by valves as shown, which can be opened or closed to obtain the flow desired,

The still I!) will be filled with the feed stock, cold light aviation gasoline for example, to which heat will be applied by admitting steam at a constant rate to the heating coil l3. vaporization of the feed will boil off hydrocarbon fractions progressing from light to heavy, and these will be totally condensed by condenser 22, and the rate of return of condensate as reflux will be regulated by the amount of condensate removed from the system as product through line 28. Control means are provided to regulate automatically the rate of condensate removal by temperature indication, and to duplicate the products withdrawn on succeeding runs.

The automatic control system is supplied with electric current from A. C. power line LlLZ, Fig. 3. In general, the control system for the distillation unit includes the following: A thermometer resistance bulb'55 at the top of the column, or in the line through which vapor is conducted from the column, is connected to a Wheatstone bridge shown in Fig. 4, which is employed to measure temperature and to determine when the temperature of the-vapors-has reached predetermined temperatures at which the reflux ratiois tobe changed or the unit cuts are to be changed from the procluction of one product to the production of the next succeeding product. Another thermometer resistance bulb 56 at the top of the column, (Fig. 2) or in the line through which vapors are withdrawn from the column, is utilized as a means of compensating the response of bulb 55 for variations in pressure within the distillation unit. Bulb 58 is electrically connected with a pressuretemperature compensating device 51, part of which is shown in Fig. 6 which serves the double purpose of compensating for temperature as well as for pressure, so that the response of the bulb 55 to temperature within the distillation unit is properly corrected for pressure other than normal atmospheric pressure, which is used as the basis for temperature settings on slide wire devices in the Wheatstone bridge, The heat supplied to the charge in the still is controlled by controlling the pressure and quantity of the steam supplied to coil I3 so that the rate of heating of the charge in the still will be substantially constant. The pressure controller 58 (Fig. 2) controls the pressure of the steam supplied to the heating coil and a flow controller 59 controls the quantity of steam supplied. The distillation unit is provided with a safety device so that should the steam pressure drop below the set point of the pressure controller 58, a pressure controller 60 will cause an alarm 6| to be sounded and will cause the distillation unit to be shut down automatically, otherwise unsatisfactory products might be produced during the period when the steam pressure was below the predetermined operatin pressure. Another safety feature employed is a high still pressure regulator 62 which, in the event the still pressure exceeds a predetermined point, operates to sound the alarm 6| and automatically shuts down the distillation unit. In the event of power failure or instrument air failure, the distillation unit is also shut down and a suitable alarm is sounded. If the unit is shut down as a result of high still pressure, the control mechanism locks up so that the unit cannot be started again without adequate attention of the operator. If the unit is shut down automatically for other reasons, the unit starts up automatically upon the restoration of the proper conditions. A pressure controller 63 is provided which operates to vent the unit to the refinery gas system in the event the pressure within the unit tends to rise above the predetermined set pressure. There is also provided another pressure controller 64 which functions to admit either isopentane vapor or refinery gas intothe unit,depending upon the stage of the operation, whenever the pressure within the unit tends to drop below a predetermined set minimum operating pressure. This latter pressure is set slightly higher than the setting of a vacuum vent safety valve on the still l0, and the controller 63 is set slightly lower than the safety controller 62 which in turn is set slightly lower than the safety valve on the still. Slop valve 42 provides means for purging the product lines of heavy distillate remaining at the end of the previous run, and the slop valve 48 serves as a means for returning to the feed tank, the small amount of improperly fractionated distillate that occurs between successive products as a result of the quantity of liquid and vapor which always remains in the fractionating column and overhead refluxing system which cannot be properly fractionated and is commonly called hold-up.

More specifically, the thermometer resistance bulb 55 in the vapor line 2! is connected through lead id in one side of a Wheatstone bridge, connecting to a fixed resistance 1|, Fig. 4, and through lead 72 to and through the temperature-pressure compensating device 5'? to be described hereinafter in detail, to lead 13 to one pole of a galvanometer M, and through lead to a fixed resistance 16. The Wheatstone bridge also contains fixed resistances 11, 18 and 7B in series with each other and a slide wire 80 in parallel with a fixed resistance 8!. The slider 82 of the slide wire 80' is connected through a single pole double throw switch 83 through lead 84 and a step switch to be described hereinafter and through lead 85 to the other pole of the galvanometer 'M through a single pole double throw switch 86 which serves to cut the galvanometer out of the circuit. The slide wire 89' together with the slider 82 and the resistances H, 18, i9 and Bi and switch 83, constitute one of twenty-four such units which are connected in parallel in the Wheatstone bridge and are mranged to be individually and successively connected in and disconnected from the Wheatstone bridge by the step switch mentioned. A fixed resistance 8'! is connected in parallel with the galvanometer. A lead 88 connects the fixed resistances H and 17 and a lead 89 connects the fixed resistances it and 19. Connected between leads 88 and 89 are the release coils 90 and 9! in series, and also connected between leads 88 and 89 are holding coils 92 and 93 in series. Current is supplied to the Wheatstone bridge from the power line LiLz through a rectifier fi l providing preferably a 6 volt D. C. potential across the Wheatstone bridge. Fixed resistances 95 and at opposite sides of the rectifier 94, serve to regulate the current flowing through the Wheatstone bridge. The Wheatstone bridge is so arranged that when the switch 83 is in position to connect lead 84 to the resistances TI and 18, the total of resistances l8, l9 and 8! and slide wire 30 will be sufficiently greater than that of Ti, so that the galvanometer '14 will deflect to high position and the step switch mentioned will cause the slide wire then in the Wheatstone bridge to be cut out of the circuit, as will be described hereinafter.

The control system is provided with thirty-five control points, twenty-four of which have individual slide wires, like slide wire 80 with resistances like ll, 18, T9 and BI, and switch 83,

iii. points associated with disc i5! and which are 6 which may be connected in the Wheatstone bridge as desired. These slide wires are connected in parallel as shown in Fig. 3, they are designated to 80 respectively, and they are individually connected to and disconnected from the galvanometer 74 by means of a rotary step switch designated generally 91, Fig. 4. Each slide wire should have a definite temperature range, thirty degrees Fahrenheit for example, and should be graduated so that the control points can be set by positioning the sliders 82, preferably to within 0.1 F. The range of each succeeding slide wire overlaps with each preceding slide wire so that the total range of the control system is covered completely.

The rotary step switch 9! comprises five discs NH, W2, W3, H54 and IE5 respectively, fixed in spaced relationship on a shaft I06, and each having a sliding contact with some point in the electric circuit of the control system and an electric contact brush which may be moved into and out of contact successively with the thirtyfive control points of the system. The shaft N16 is rotated step by step by means of a ratchet I01 and a pawl I08 which is actuated by a solenoid 509, the circuit to the coil of which is controlled by a mercury switch H0, the mechanism for actuating which at the proper times will be described hereinafter.

Disc Hill which functions to connect the slide wires and the holding coils 92 and 93, successively into the Wheatstone bridge and to disconnect them from the bridge, is connected to the galvanometer M through lead and sliding contact In addition to the twenty-four control numbered 1 to 24 inclusive, there are eleven other points designated Ts, Ts, To, 4, '7, 10", 13, 16, 19, 22 and 25. A lead line H2 connects with each point 4', '7', 10', 13, 16', 19, 22' and 25', and each lead i 92 connects through a single pole, single throw switch H3 and a lead M4 to a common connection H5 which is connected through lead H6, through points To, Ts and TE, and lead ill to a point 4!! between the holding coils =92 and 93. The switches H3 are operated simultaneously with corresponding switches 83. A brush H8 on the disc IEH is positioned to be moved into and out of contact successively with the thirty-five control points.

Disc N32 is connected to power line L1, through a lead H9 through a sliding contact 12!]. The disc IE2 is provided with a brush l2] which is positioned to be moved into and out of contact successively with thirty-five control points corresponding to, and designated the same as, the control points associated with the disc llil. Each of control points 1 to 24 inclusive is connected to an electric lamp of the same number. The points 4', 7, 10', 13, 16', 19' and 22 have no lamps, but are connected respectively to points 4, 7, 10, 13, 16, 19 and 22. Point 25' has no connection. Each point To, Ts, and TE is also connected to a lamp correspondingly numbered. Lead l22 connecting one side of all the lamps l. to 24 inclusive is connected to a lead I23 which connects with one side of the lamps To, Ts and TE and to power line L2. Point TE also is connected by lead M4 to a manually operated push button l25. Point Ts is also connected by a lead I26 to a manually operated push button l2l.

2&3 functions to vary the reflux rate to the column i9 as required at diiTerent stages of operation of the distillation unit. Disc m3 is connected to power line L1 through sliding contact I28 and leads I28 and I30, relay R4, lead 222, emergency switch 223 by means of which the distillation unit may be shut down completely in the event of any emergency requiring shut down, lead 213, mercury switch 21I and lead 212. This disc is provided with a brush I32 which is positioned to be moved into and out of contact successively with thirty-five control points corresponding to, and designated the same as, the control points associated with the discs IOI and I02. Control points To, 1, 4, 4, '1', 1, 10, 13, 13, 16, 16, 19, 19, 22', 22 and 25 are connected together as shown in Fig. 3. Control points 2, 5, 8, 11, 14, 17, 20 and 23 are also connected together as are control points 3, 6, 9, 12, 15, 18, 21 and 24.. Point 1 is connected by a lead I33 to the operating coil of a solenoid operated valve I34 in air line I35 connected at one end to an air line I36 and at the other to the control setting mechanism of a flow recorder controller I31 which receives its operating power from air line I36, and which is of any suitable type such as the Foxboro type. Controller I31 is connected to an orifice member I38 in product line 30, and controls the position of a valve I39 in the product line 30. A valve controlled by-pass I40 is pro vided around valve I39. The other side of the coil of valve I34 is connected to power line L2 through leads MI and I42. Point 2 is connected by a lead I43 to one side of the operating coil of a solenoid operated valve I44 in air line I45 which connects with air lines I35 and I36. The other side of the coil is connected to lead I42 by a lead I46. Point 3 is connected by a lead I41 to one side of the operating coil of a solenoid operated valve I48 in an air line I49 extending between air lines I35 and I36, the other side of the coil being connected to lead I42 by lead I50. A pressure reducing valve I5I is disposed in each air line I35, I45 and I49 ahead of the control valve therein and each line is provided with a pressure gage I52. An electric lamp I53 is connected in parallel with each of the coils of the valves I34, I44 and I48, and each lead I33, I43 and I41 is connected through individual switches, with a lead I54 which is a branch of power line L1, permitting manual operation to energize the coils of valves I34, I44 and I48. The operation is such that the valves I34, I44 and I48 function to admit difierent predetermined air pressures to the control setting mechanism of the flow recorder controller I31 thereby to set the control points of the controller to provide three different settings of valve I39 and three different rates of flow through the product line 30 with consequent difierent rates of flow of reflux down column I9.

Disc I04 provides means for opening the proper product valve depending upon the stage of the operation of the distillation unit. Disc I04 is connected to power line L1 through sliding contact I55 and leads I56, I29 and I30, relay R-4, lead 222, emergency switch 223, lead 213, mercury switch 21I and lead 212. This disc is provided with a brush I51 which is positioned to be moved into and out of contact successively with thirty-five control points corresponding to, and designated the same as, the control points associated with the discs IOI, I02 and I03. As shown in Fig. 3, points 1, 2, 3 and 4' are connected together, points 4, 5, 6 and '7' also are connected together, and each succeeding group of four points are connected together. Point TE is connected by lead 226 to the release coils of relays R4 and lit-5. Points Tn, Ts and T0 are not connected to any other control point. Points 1, 2, 3 and 4' are connected by lead I58 to the operating coil of a solenoid operated valve I59 in an air line I63 to the diaphragm of a valve I6I which controls product line 3| through which the first cut is removed from the distillation unit. When the solenoid is energized, valve I59 opens and permits air to flow to the diaphragm of valve I6I and to open it against the action of a spring which closes the valve when the solenoid is deenergized and allows the air to escape from the diaphragm. The other side of the solenoid coil is connected through leads I52 and I63 to a contact point of a relay R-1 which is arranged for mechanical lock-up, and to lead 233, to a time delay device TD2 and lead I88 to power line L:. Each of the other successive groups of four control points associated with the disc I04 is connected by a lead like lead I58, to the operating coil of a solenoid valve which controls the admission of air to the diaphragm of a product valve, like valve I6I, in each of the product lines 32 to 33, as clearly shown in Figs. 2 and 3. An electric lamp I64 is connected in parallel with the solenoid of the valve I59 for each product line. Each lamp is connected to power line L1 by a lead I65 having a switch I66 permitting manual operation to energize the coils of valves I59. The point To associated with disc I04 is connected through lead I61 to a time delay device TDI of any suitable type for the purpose, such as the Vernier-set timer manufactured by the Automatic Temperature Control 00., Philadelphia, Pa.

Disc I05 provides means for operating the slop valves 42 and 48 and for controlling the opening and closing of the iso-pentane and refinery gas admission valves 208 and 205 and also for setting the control point of the column pressure regulator 63. Disc I05 is connected to power line L1 through a sliding contact I68 and leads I69, I29 and I30, relay R-4, lead 222, emergency switch 223, lead 213, mercury switch 2H and lead 212. The disc is provided with a brush I10 which is positioned to be moved into and out of contact successively with thirty-five control points corresponding to, and designated the same as, the control points associated with the discs IOI, I02, I03 and I04. Points 4, 7', 10, 13', 16', 19', 2.2, and 25' are connected together. No other point is connected to any other point. Point 4' and the other points connected to it, are connected through lead I1I to a time delay device TD2 similar to TD-I. Point 4 is connected through lead I12 to the release coil of a relay Rr-I having a mechanical lock-up. Point '1 is connected through lead I13 to the operating coil of a relay R8 having a mechanical lock-up. Point T1: is connected through lead I14 to the operating coil of relay RI and to the release coil of relay R8.

Time delay mechanism TD-I functions to hold slop valve 42 open to permit a purging of the product line 26, pumps 21, product line 28, cooler 29 and product line 30 at the beginning of the run. TDI is connected to power line Ll through a lead I15, and it is connected through lead I16 to the operating coil of a solenoid valve I11 which controls the supply of air to the diaphragm of slop valve 42, the 0011 also being connected through lead I18 to power line L2. An electric bulb I19 is connected in parallel with the coil of the solenoid of the valve I11. Lead I16 is connected through a switch I and a lead IN to power line L1. TD-I is also connected through lead I82 to the operating coil of relay R6, through lead I85 to power line L2, through lead I86 to a contact point of relay R9 having an electrical lock-up, and through lead I61 to point To associated with disc I04.

Time delay mechanism TD-2 functions to hold a valve in a product line open, after the temperature within the column has reached the set point, for a sufiicient period of time to permit the product then leaving the column to reach that valve. TD2 is connected through lead 233 to a contact point of relay R1 and through lead I81 to the operating coil of relay R-1, through lead I 88 to power line L2, and through lead Hi to control point 4 associated with disc I05.

Time delay mechanism TD-3, similar to TDI and TD2, functions to close the product valve which is open at the end of a cut and to open slop valve 48 for a sufficient period of time to permit slopping of the unsatisfactorily fractionated distillate which results from the hold-up of the column. TD-3 is connected through lead I89 to the operating coil of a solenoid valve I90 which controls the supply of air to the diaphragm of the slop valve 48, the coil also being connected through lead I9I to lead I18 and to power line L2. A lamp I92 is connected in parallel with the coil of the solenoid of valve I99. Lead I89 also is connected through a switch I93 with lead I8I which connects to power line L1. TD-3 also is connected through leads I94 and I84 to the release coil of relay R- I and through leads I94, I88 and I82 to the operating coil of relay R-fi, through lead I95 to power line L2, through leads I95 and I81 to TD2, through leads I91, I3I, I32, relay R-4, lead 222, emergency switch 223, lead 213, mercury switch 21I and lead 212 to power line L1, and through lead I99 to the operating coil of relay R-1.

Relay R-I which is provided with a mechanical lock-up, has one side of the operating coil connected to point TE of disc I by lead I14 the other side of the coil being connected by lead sec to power line L2. The release coil of this relay is connected on one side to lead I12 to point 4 of disc I85 and on the other side by lead 459 to power line L2. Relay R-I contact points are connected by leads 292 and 222, emergency switch 223, lead 213, mercury switch Z'II and lead 212 to power line L1, and through lead 203 to the operating coil of a solenoid valve 254 which con trols the admission of air to the diaphragm of valve 255 which is arranged to be opened by a spring upon failure of the air supplied through the valve 284 to the diaphragm, Relay RI is also connected through lead 296 to the operating coil of a solenoid valve 201 which controls the supply of air to the diaphragm of the isopentane valve 293 which is arranged to be closed by a spring upon failure of air to the valve 291 and to the diaphragm.

The operating coil or relay R-Z is connected through lead 299 to push button I25 and through lead 2c! to the power line L2. Relay R-2 contact points are connected through leads 2m and 2H to the release coils 99 and 9! of the Wheatstone bridge, and through leads 2I2 and 2I3 to lead 85 extending between the galvanometer 14 in the Wheatstone bridge and the disc I9I.

.he operating coil of relay R3 is connected by lead 2M to one side of push button I21 and through lead 2I6 to power line L2. The operating coil is also connected through contact points and leads 2| 5 and 2I5' in parallel with push button I21 so that the relay locks up electrically 10 after the operating 'coil is once energized. An-" other set of contact points connects the galvanometer M to the release coils 99 and 9| at point 452, through leads 2I1, 2I3 and 85, and 2I8 and 2. Relay R-3 contacts also connect power line L2 by lead 2H6 through leads 289 and 220 to the operating coil of R-4.

Relay R-d which is provided with a mechanical lock-up has one end of the operating coil connected through lead 220 to power line L2 as described above, the other end of the coil being connected-through lead 222, emergency switch lead 213, mercury switch 21I and lead 212 to power line L1. The release coil of relay R-4 connected on one end through lead 225 and lead with point TE on disc I04 and also to the high still pressure control relay contact point through. lead 28, while on the other end it is connected to power line L2. relay R-t connect line 530 through lead 222, emergency switch 223, lead 213, mercury switch Elli and lead 212 to power line L1.

The operating coil of relay R-5 is connected through lead 228 to the push button 229 through the push button, lead 235 and throughlead I30 to power line L1 as above, the other end of the coil is connected to power line L2. The operating coil is also connected through contacts to lead 23!! and to lead 23I which is connected to 839 causing the relay to lock up electrically. This relay also has a mechanical lock up the release coil of which is connected in parallel with the release coil of relay R-d by lead 224 and the extension of ower line L2. The contact points of relay R-5 are connected as above to lead I39 and also through lead 242 and lead 246 to push button 2 559 and through lead 243 to the starting equipment 242 for the motors for product pumps 21. The pump starter mechanism is connected to main line L2 through lead 245.

Relay R6 has its operating coil connected through lead I82 to time delay mechanisms TD-I and TD 3 and through lead 232 topower line L2. Relay R 6 contact points are connected through leads 2, 2!!! and 2 to release coils 9i! and 9! at point M2 and through leads 2I5, 2I2, M3 and 85 to galvanometer 14.

The operating coil of relay R-1 which is provided with a mechanical lock-up, is connected through leads I8! and I96 to time delay mechanisms 'ID-2 and TD- 3, and through lead I 99 to time delay mechanism TD-3. The release coil of relay R-I is connected through leads I84, I94, l83 and I92 to time delay mechanisms TD-I and TD-3 and to relay R-5, and through lead 234 to power line L2. Relay R-1 contact points are connected through lead I63 to the coils of the solenoid valves which control the supply of air to the product valves I GI and through lead 233 to time delay mechanism TD-Z.

Relay R-8 which also is provided with a mechanical lock-up, has the operating coil connected through lead I13 to point 7 associated with disc I05, and to power line L2 through lead 235. The release coil of relay R8 is connected through lead 238 to power line L2 and through lead 200 and lead I14 to point TE of disc I95. Relay R8 contact points are connected through leads I29, I32, etc. to power line L1 and through lead 236 to the solenoid valve 231,

Relay R-9 which is provided with an electrical lock-up has its operating coil connected through lead 239 to push button 240 and through lead 24I the contact points connected to lead 242 in paral- The contact points of to power line L2 and is locked up through lel with the push button. The contact points also connect the power line L2 through lead 24! and lead !86 to time delay mechanism TD-!.

The pressure of steam supplied to heating coil !3 in still I!) is controlled by a diaphragm operated valve 241, Fig. 2, spring pressed to closed position which is by-passed by a valve controlled by-pass 248. Air is supplied to the diaphragm of valve 241 through air line 249 which is controlled by pressure indicator controller 56 connected by air line 259 to the steam line !4. The pressure indicator controller may be of any suitable type, such as that supplied by the Foxboro Company. The quantity of steam supplied through steam line !4 to the heating coil !3 is controlled by a diaphragm operated valve 25! in line I4, spring pressed to closed position which is by-passed by a valve controlled by-pass 252. Air is supplied to the diaphragm of valve 25! through air line 253 which is controlled by flow recorder controller 59 of any suitable type such as that supplied by the Foxboro Company of Foxboro, Mass. The controller 59 is connected to an orifice member 254 in the steam line !4 between Valves 241 and 25!. A'three-way solenoid operated valve 255 is disposed in air line 253 between controller 59 and valve 25!. Valve 255 is operated by a solenoid 256 admitting air to the diaphragm of valve 25! when the solenoid is energized and venting the diaphragm to the atmosphere when the solenoid is deenergized. The coil of solenoid 256 is connected by a lead 251 to power line L2 and by a lead 258 to lead l3!. An electric lamp 259 is connected in parallel with the coil of solenoid 256 and is also connected 1:.

through a switch controlled lead 260 to leads 22 I, 222, emergency switch 223, etc. to power line L1. The arrangement is such that when solenoid 256 is deenergized, the flow of air to valve 25! is cut off and it is moved to closed position thereby 4% cutting off the supply of steam to the still I 8. Solenoid 256 is deenergized to cause valve 25! to be closed on (1) completion of the batch distillation, (2) on power failure, (3) on low steam pressure, (4) on high still pressure and (5) on any other emergency shut down. Valve 25! closes due to loss of air pressure on air failure.

Pressure controller 60 of any suitable type such as supplied by the Foxboro Company, is connected to the steam line !4 through conduit 26! ahead of valves 241 and 25!. Controller 68 controls the air supplied through line 262 to a, pneumatically operated mercury switch 263 normally open, which is connected through lead 264 to power line L1 and through lead 265 to the operating coil of a relay 266 which also is connected through lead 261 to power line L2. Relay 266 when energized, closes a circuit including howler 6! and an electric lamp 269 connecting these through the relay contact points, lead 268, switch 263 and lead 264 to line L1, both the howler and the lamp being also connected to line L2. Controller 68 also controls the supply of air through line 210 to a pneumatically actuated mercury switch 21! normally closed, which is connected through lead 212 to power line L1 and through lead 213 to emergency switch 223. The controller 68 is provided with a limit lock-up head and two set pointers which function to prevent the distillation unit from starting up after it has been shut down because of lowpressure, until the steam pressure has regained a pressure slightly above the minimum operating pressure. The arrangement is such that when the steam pressure supplied to the heating coil in the still falls below 12 the determined pressure, switch 263 will be closed, and relay 266 will be energized thereby closing the circuit including howler 6! and light 269. Simultaneously switch 21! is moved to open position thereby breaking the power circuit to the unit and shutting down the unit. Simultaneously the product and slop valves are closed, the steam supplied through line I4 is shut off through the operation of controller 59, and the product pump 21 is shut down. When the steam pressure is returned to the predetermined minimum pressure, performance is restored automatically at the point where it was interrupted so that no cycle is repeated.

Still pressure controller 62 of any suitable type such as that supplied by the Foxboro company is connected to still I8 through a pressure transmitting line 214 which is controlled by a valve 215. Controller 62 controls the flow of air through an air line 216 to a pneumatically actuated mercury switch 211, normally open, which is connected by lead 218 to a relay 219 the operating coil of which is also connected by leads 288 and 28! to power line L2. Switch 211 is connected by lead 282 to power line L1. An electric lamp 283 is connected in the circuit closed by the relay 219 contact points, and in parallel with the howler 6!. The contact point for the lamp is also connected by leads 226, 225 and 224 to the release coils of relays 55-4 and R-5. The arrangement is such that when the pressure in still I!) exceeds a predetermined pressure, controller 62 will cause switch 21'! to be closed thereby energizing relay 219 and closing the circuit through howler 6 I, lamp 283 and the release coils of relays R4 and R-5. The opening of relays R-4 and R-5 prevent the unit from starting automatically after the high pressure in the still has been reduced. When the pressure in still !8 exceeds the predetermined pressure, the controller 62 functions to close the product valves and the slop valves to shut off the steam supplied to the heating coil in the still by the operation of controller 59, and to shut down the product pump 21 then in operation. The unit is put back in operation by pressing reset button !98 which causes relay R-4 to close, reopening the steam control valve 25!, product valves etc. and by then pressing button 229 closing relay R--5 restarting the product pump.

The air failure alarm includes a pneumatically actuated mercury switch 284, normally open, which is connected to air line 285 which in turn is connected to the source of instrument air for the unit. Switch 284 is connected to power line L1 by lead 286 and by a lead 281 to a relay 288 which is connected through lead 289 to power line L2. Relay 288 closes the circuit of an electric lamp 299 and lead 29! which is connected to the circuit containing howler 6!. Upon failure of instrument air, switch 284 will be closed, thereby energizing relay 288, causing lamp 298 to light and howler 6! to sound. At the same time the product valves and slop valves are closed and the supply of steam to the heatin coil in the still is shut off through the action of control valve 25!. When the air supply is regained, the performance of the unit is automatically restored at the point at which it was interrupted so that no cycle is repeated.

In the event of power failure, the solenoid 293 of a solenoid valve 292 is deenergized, this solenoid being connected to power lines L1 and L: by leads 294 and 295. On being deenergized, the valve opens air line 296 and air is supplied to an air whistle 291. Upon power failure the product valves and slop valves are closed, the steam supplied to the heating coil of the still is shut off through the action of control valve 251 and the product pump 21 then in operation is shut down. On regaining the power supply, the performance of the unit is automatically restored at the point at which it was interrupted so that no cycle is repeated.

The vapor space of condenser 22 is connected through line 298 to a line 299, one end of which is connected to a source of isopentane vapor or refinery gas, and the other end of which is connected with the gas recovery system of the unit. Pressure indicator controller 54 of any suitable type such as supplied by the Foxboro Company, is connected to line 299 through line 300 so that variations in pressure of the vapor in line 299 will be transmitted to the controller 04. Controller 64 controls the air supplied in a line 301 to the diaphragm of a valve 302 in line 299 at the left of the juncture of lines 298 and 299, as seen in Fig. 2. Valve 302 is by-passed by a valve controlled by-pass 303. When the pressure in the line 299 and the distillation unit falls below a predetermined pressure, such as atmospheric pressure, controller 64 will operate to open valve 302.

Pressure indicator controller 63 which in this instance has two control points, has one point set for one-half pound and the other for ten pounds pressure, and is connected to line 299 through line 304. Controllers of this type are also supplied by the FoXboro Company. Controller 63 prevents the pressure in the distillation unit from exceeding the set pressures by opening the diaphragm valve 399 whenever the pressure in the line 299 rises above the set pressures. Valve 306 is by-passed by a valve controlled by-pass 301. Air lines 308 and 305 connect controller 63 with valve 231 which also connects to the air line 306 leading to the diaphragm of valve 306. Valve 231 is a three-way valve arranged so that air pressure may be transmitted to the diaphram of valve 306 so as to control the pressure in line 299 at either set point as desired. Valve 231 is actuated by a solenoid 309 which is connected through lead 310 to power line L2 and through lead 236 to relay R6. An electric bulb 3| 1 is connected in parallel with the coil of solenoid 309 and the lamp is connected through a switch controlled lead 312 to power line L1. In operation, with the distillation unit under pressure of isopentane vapor, when the still is charged with light aviation gasoline for example, the vapors in the unit will be compressed to about ten pounds unless the excess pressure is relieved by condensation of some of the isopentane vapors. When heat is admitted to the still and the feed begins to vaporize, it will be necessary to vent gas to keep the pressure down to ten pounds. When the temperature control point '7 is reached the control system will be reset automatically to open at one-half pound pressure by operation of the three-way solenoid operated valve 231, the position of the valve being indicated by the signal lamp 311.

A refinery gas admission line 313, has one end connected to vapor line 299 and the other end connected to the refinery gas system. Line 313 is controlled by valve 205 which is arranged to be spring pressed to open position and to be closed by a diaphragm to which air is supplied through a line 314. Valve 295 is by-passed by Valve controlled iine 313. Air line 314 is controlled by valve 204 which is actuated by a solenoid 315, the coil of which is connected by lead 316 to power 14' line L2, and is connected by lead 203 to relay Rf. A signal lamp 311 is connected in parallel with the coil of solenoid 315, and this lamp is connected to power line L1 through a switch controlled lead 316. In operation, valve 205 normally is open, and in the event the pressure in the distillation unit drops below the predetermined pressure, controller 64 will cause valve 302 to open and to admit refinery gas into the unit through line 313. Signal lamp 311 will indicate when valve 205 is open.

The supply of isopentane vapor to vapor line 299 is controlled by valve 203 which is spring pressed to closed position and which is actuated by a diaphragm to which air is supplied through line 319. Valve 208 is by-passed by valve controlled by-pass 320. Air line 319 is controlled by a valve 201 which is actuated by a solenoid 321, the coil of which is connected by lead 322 to lead 206 which connects with relay R1, and by lead 323 to power line L2. A signal lamp 324 is connected in parallel with the coil of relay 321 and is connected through a switch controlled lead 325 to power line L1.

Thermometer resistance bulb 56 is connected by a lead 326 to one end of a slide wire 321, Figs. 4 and 6, in the temperature-pressure compensator 3'1, and by a lead 328 to a fixed resistance 329 which is connected through a lead 330 to the other end of a slide wire 321. Slider 331 of slide wire 3121 is connected through lead 13 to the galvanometer E4 of the Wheatstone bridge. Slider 331 is arranged to be moved in response to variations in pressure within the distillation unit by means of the mechanism shown in Fig. 6. The pressure of the vapors leaving the column 19 and variations therein are transmitted by a conduit 332 shown in Fig. '6 but not in Fig. 2, to a pressure measuring device comprising a manometer 333 partially filled with mercury 334, one leg of which is connected to a vacuum pump through line 335, and

the other leg of which has a float 336 which actuates a gear segment 331 on a shaft 338 to which is fixed one end of a link 339, the other end of which is pivotally connected to one end of a link 340, the other end of which is pivotally connected to the lower end of an arm 341 pivoted at 342. A flapper 343 also pivoted at 342 is maintained in fixed relationship to arm 341 by an extension 344 on arm 341. The upper end of arm 341 is adjustably connected by suitable means 345 to the upper end of an indicating arm 346 which also is pivoted at 342 and moves over a scale 341. Flapper 343 regulates the flow of air through a nozzle 348 which is pivoted at'342 and to which air is supplied through flexible air line 349, the other end of which is connected to a bellows 350 to which is connected a pilot valve 351. A pointer 352 fixed to the nozzle '348 and pivoted at 342, also moves across scale 341. Pilot valve 351 moves in a housing 353 having a valve seat 354 and an opening 355 to the atmosphere, and an op: positely disposed seat 356' on a threaded plug 351 which is adjustable with respect to the housing 353 and the valve 351. The valve seat end of the plug 351 has an axial bore 358 and a connecting radial bore 359 which connects with an air passage 360 to which air is supplied through line 331, filter 362, line 363, pressure reducer 364 and line 355. A gage 366 measures the pressure of the air supplied to the device. An air line 361 has one end connected to the air passage 360 and the other end connected to air line 349, and has a reducing tube 368 therein. Valve chamber 369 is connectedwith an air passage 310 which is also connected-throughair line 311 to a diaphragm motor 312. A gage 366' measures the pressure of the air supplied to the motor 312. The diaphragm 313 of motor 312 is urged in an upward direction by a spring 314 and in a downward direction by the pressure of the air supplied through line 31!. The diaphragm is connected through a strap or chain 315 to the periphery of a disc 316 fixed to a shaft 311 which is urged in a counter-clockwise direction, as viewed in Fig. 6, by a torsion spring 318 having one end fixed to a stationary point. The slider 33! of slide Wire 321 is also fixed to the shaft 311 and is electrically connected to lead 13 by a wire 319. A cam 399 is mounted on shaft 311 in such manner that the angular position of the cam with respect to the aXis of the shaft may be varied by a suitable adjusting mechanism including an arm 38! having one end fixed to the shaft 311 concentric with the axis of the cam, a stud 382 which is fixed to the cam eccentrically with respect to the shaft and a link 383 which extends between the outer end of arm 38! and the stud 382, the arrangement being such that adjustment in the effective length of the link 333, will vary the angular position of the cam with respect to the shaft 311. A follower 384 on the end of an arm 335 which is pivoted at its other end at 342 is fixed to the nozzle 348, causes nozzle 348 to swing about the pivot 342 upon movement of the shaft 311 by the motor 312. A spring 386 urges the cam follower into contact with the periphery of the cam. The operation is such that the float 339 operates the flapper 343 and the flapper regulates the flow of air through the nozzle 343 to control and to position the pilot valve 35! which in turn regulates the displacement of the diaphragm motor 312. The diaphragm motor produces the force which is necessary to actuate and position the slider 33! on the slide wire 321 in accordance with the periphery of the cam 389, which operates to reposition the nozzle 349 to effect a condition of equilibrium. It will be understood that a decrease in pressure in the distillation unit will movethe flapper away from the nozzle thereby diminishing the pressure in bellows 359 and causing pilot valve 35! to move toward or to be seated on seat 3554 thereby increasing the air pressure on the diaphram 313, moving the cam in a counter-clockwise direction, as viewed in Fig. 6, and moving the nozzle 348 toward the flapper to efiect equilibrium. Increase in pressure in the distillation unit will have the opposite effect upon the pressure temperature compensating mechanism. In consequence, slider 33! will be moved with respect to the slide wire 321 in response to variations of pressure within the distillation unit, the extent of such movement being determined by the shape of cam 389. The resistance of slide wire 321 and the resistance 329 are so proportioned that when the pressure within the distillation unit is that of normal barometric pressure, the resistance of that portion of slide wire 321 to the left of the slider 33!, as viewed in Fig. 4, will be exactly equal to the sum of resistance of that portion of the slide wire 321 to the right of the slider, as viewed in Fig. 4, and the resistance of fixed resistance 329, in consequence of which there will be no compensation regardless of the temperature within the distillation unit. However, when the pressure within the distillation unit is other than normal barometric pressure, slider 33! will be in contact with some other point in the slide wire 321, as a result of which the resistance on one side of the slider will be different from that on the other side, which will have the effect of placing a greater portion of the resis tance of thermometer resistance bulb 59 on one side of the Wheatstone bridge than on the other, thereby influencing the balance point of the galvanometer 14 and compensating the resistance of the thermometer resistance bulb 55 for deviation of the pressure within the unit from normal barometric pressure.

One means for moving the mercur switch !!9 to closed position at the proper times and thereby moving the step switch 91 step by step, is shown in Fig. 5. Alternating current motor 399 which is connected across the power lines L1 and L2, continuously drives a cam 39! which is fixed to a shaft 392 that is driven by the motor through suitable speed reducing mechanism, not shown. A chopper bar 393 fulcrumed at 394 has a cam roller 395 at one end which is urged into contact with the periphery of cam 39! by a spring 393. The other end of the chopper bar is provided with a roller 391 which engages one end portion of a switch operating lever 398 which is pivoted at 399 to a fixed point 499, the other end of the lever 398 being provided with the weight 49! which urges the lever in a counter-clockwise direction, as seen in Fig. 5. Lever 398 actuates mercury switch H9 in such manner that when the lever is in the position shown in Fig. 5, the mercury switch is closed, and when the weight end of lever 398 is in contact with or adjacent the stop pin 492, the mercury switch will be inclined with its right hand end above its left hand end, or in the position shown in Fig. 3, and the switch will be open. Switch H9 is connected to power line L2 and through lead 493 to the coil of solenoid I99 and to power line L1 which actuates pawl !98 and moves the ratchet !91 which is fixed to shaft !99 of the step switch 91. Switch protecting means 494 is interposed between the mercury switch and the operating lever 398.

The chopper bar 393 is provided with a downwardly extending skirt 495 intermediate the fulcrum 394 and the roller 391. The chopper bar is associated with the galvanometer 14 and with the galvanometer needle 496 which is suspended in the usual manner by a suspension wire 491 with which is associated an electromagnet 498 disposed between the poles of a permanent magnet 499. The galvanometer scale is designated 4I9. It will be understood that as shown in Fig. 5, the galvanometer needle extends in a direction normal to the plane of Fig. 5. The arrangement is such that as the temperature in the distillation unit measured by thermometer resistance bulb 55 approaches the temperature for which the particular slide wire 89' to 99 then connected into the Wheatstone bridge is set, the galvanometer needle will move from the low point or left hand side toward the balanced position which is indicated in Fig. 5. When the galvanometer needle indicates a low temperature, part of the needle will be positioned directly under the skirt 435 of the chopper bar 393 and will prevent the chopper bar from closing mercury switch H9. So long as the galvanometer needle indicates a low temperature condition for the particular out being taken off from the fractionating column, the skirt of the chopper bar will come in contact with the galvanometer needle and will prevent the chopper bar from moving to the position shown in Fig. 5 at which the mercury switch H9 is closed, and the galvanometer needle will permit the chopper bar to move downwardly to. the position shown in Fig. 5 only when the galvanometer needle has moved to balanced 17 position or to the high side to the right of the balanced position. When the needle prevents the closing of switch I II), the chopper bar will pivot about the galvanometer needle and not about the fulcrum 394.

The operation of the distillation unit and the controls is as follows: Until indicated otherwise, the description to follow will describe the steps to be taken to place the unit in condition to begin the batch distillation. Each of the slide wires 80' to 80 inclusive is set for the maximum temperature at which some action in the control of the distillation unit is to take place, these temperatures being set at successively increasing temperatures at which these actions are to occur automatically. Relay R--I is in locked position which results in supplying power to solenoid 32I which controls valve 298 in the vapor line 299, thereby opening valve 288 and lighting signal lamp 324, in consequence of which isopentane vapor is admitted, through lines 299 and 298 into the condenser and into the fractionating column I9, whenever the pressure in the tower drops lower than a predetermined pressure such as onehalf pound per square inch below atmospheric pressure. Pressures in the tower lower than this will result in the opening of pressure control valve 302.

At this point, each of the discs Ifll to I95 inclusive of the step switch 91 has its brush at point TE, and the galvanometer I4 is connected to point 4 intermediate resistances 92 and 93 of the Wheatstone bridge, which results in maintaining the galvanometer needle on the low side because the relationship of resistance 92 of the Wheatstone bridge to the resistance 93 is such that when the galvanometer is connected topoint II I, there is produced the same eflect as if the slide wire 80' were set for the maximum tem- Perature. It will be understood that the resistances 92 and 93 of the Wheatstone bridge, function as holding coils to prevent the mercury switch IIII from being closed. All other relays except relay R-I, are in open position. With the brush of disc I02 on point TE signal lamp TE is lighted.

With the still iiliand the :fractionating column I9 under a small superimposedgas pressure, and with water flowing through the overhead condenser 22, light aviation gasoline for example is charged to the still. The gas which is displaced by the charge is compressed to a pressure at which some of the isopentane in the system condenses.

Push button I25 is then pushed to and held in closed position which results in the energization of the operating coil of relay R-2 and closing of the relay contact points thereby connecting the galvanometer 14 to point 4I2 of the Wheatstone bridge (Fig. 4), which causes the galvanometer needle to swing to the high position because the resistances 90 and 9I are so proportioned that connecting in these resistances has the same effect as connecting in the slide wire with the lowest possible setting. The effect of connecting coils 90 and 9I to the galvanometer is opposite to that of connecting coils 92 and 93 to the galvanometer. With the galvanometer needle in high position, the chopper bar 393 will move downwardly and close mercury switch H which energizes the coil of solenoid I09 and moves the step switch 91 one step, thereby moving the brushes of the discs vIIH to I95 inclusive from point TE to point Ts- Button Ishouldbe held in closed position until the-chopperlbar .393 can move the mercury switch III! to closed position to cause the step switch to move to point Ts. Upon movement of the step switch, TE light is extinguished and Ts bulb is lighted. Additionally, push button I2! is connected to the power line and button I25 is disconnected therefrom, thereby deenergizing relay R--2 and-disconnecting release coils and 91 from the galvanometer, holding coils 9 2 and 93 remaining connected to the galvanometer.

Button 12 is then pressed to closed position Whichenergizes the coil in relay R4, closing this relay, which reconnects the galvanometer to coils 98 and ill and simultaneously closes on electrical lock-up contact in relay 'R-3, also simultaneously closing relay R- l which looks up mechanically by means of any suitable mechanism, and supplies power to push-button 229 and to solenoid 256 of valve .255 controlling the airline to valve 25I, which turns on the steam to the heating coil l3 in still Ill under the control of flow controller -59 and lights bulb 259, and also simultaneously supplies power-t0 step switch discs 163, we and 195. As soon as the chopper bar r 393 is permitted to moveto its lowermost position and closes mercury switch Illl, step switch 91 is moved from point Ts to point To which disconnects the power from button I21 and from the electrical lock-up of the coil of relay R-B, thereby releasing an opening relay R-3 and disconnecting the galvanometer from coils 90 and 9|, holding coils 92 and 93 remaining connected to the galvanometer. Simultaneously bulb Ts is extinguished and bulb To is lighted and one side of the power line is connected to time delay mechanism TD-l. At the same time power is supplied to the solenoid of valve I36, thereby admitting air at a predetermined control pressure controlled by air -pressure reducing valve IEI to product flow record-er controller I31, thereby'setting the control point for this controller and opening controlled valve I39. Simultaneously bulb I53 is lit.

-Withsteam flowing to the steam coil I3 in the batch still Ill, the temperature of the feed will rise to the vaporization point, displaced gas in the system above the liquid will build up to an equilibrium pressure and any excess gas will be vented off through line 299 through valve 396 controlled by controller 93 at .ten pounds gage, for example. With vapors rising continuously from the still, ascending through the column I9, condensing in the overhead condenser 22, and with condensate returning through the column I9, an observation will be made of the rate of condensate returning to the still by indication of flow at flow :indicator lil. When this flow indicater :indicatesthat a predetermined rate of flow has been attained and sufiicient fluid is available in the suction of one of product pumps 21, that pump is then started by pressing push button.

switch 229 which-connects the starter equipment 2 113120 the power line. At this stage of the opera tion, pressure indicating controller 63 is set to maintain a maximum pressure of ten pounds gage. The closing of push button 229 results in the supplying of power to push button 268 and in energizing relay Rr-5 which-locks up mechanically to maintain the circuit supplying power to the motor starting equipment. Product ,pumps 2'! maybe driven byan electricmotor which iscontrolled by the combination magnetic starting switch-and ade-ion ci-rcuit breaker. The starting switch .maybemanually operatedby a startstop ,push button SWitUhyOIle located at the .pump

19 motor and one located at the switch structure. Additionally, a manual-automatic switch may be provided for each starter on the switch structure. The function of these switches is to place the starter controlling the motor either in manual operating position or in automatic operating position. Push button 229 will start the pump 2? when the manual-automatic switch is on automatic position. In order to prevent both of the pumps 21 from operating at thesame time, a 1

transfer switch may be located on the switch structure so that only one of the pumps can be operated automatically by push button 229. Product pump 21 will be startedagainst a closed discharge, vented and brought to full differential head. After the pump has been vented, one hand control valve 413 in the discharge lines from the pumps 21, is opened slowly at first and thereafter is opened wide when the operation is satisfactory. The rate of flow of product through line is controlled by the flow recorder controller i3! through valve I39. As previously mentioned, the reflux flow rate in column 19 is varied automatically as required by the stage of the distillation. This is accomplished by controlling the rate of flow of the product from the unit, thereby indirectly controlling the rate of flow of the balance of the condensate downwardly through the column 19.

The distillation unit is now ready to be put on automatic control. Push button 239 is pressed to closed position which energizes relay R-G, locking up electrically, and feeds power to timer TD-l, starting the timing operation and simultaneously energizing the solenoid of valve l'l'l which controls slop valve 42, thereby admitting air to the diaphragm of valve 42 and opening this valve and lighting bulb I19. At the expiration of the time delay period, the circuit of the solenoid of valve H1 is broken and valve li'i closed and bulb H9 is extinguished, and a second circuit in TD-l is established which energizes relay R-B thereby reconnecting the galvanometer i i to the resistance coils 90 and 9i in the Wheatstone bridge, moves step switch one step from point To to point 1, simultaneously disconnects power from 'ID-l which then resets, turning out To light, lighting point 1 light, also connecting galvanometer i l to slide wire ll, simultaneously energizing the solenoid of valve !59, controlling the air line to product valve lSl in line 31, thereby admitting air to the diaphragm of valve it! and opening this valve and lighting bulb it.

As the temperature is approached for which slide wire 80' is set, the needle of galvanometer id moves from the low point toward the balanced position and when the set temperature is reached, the galvanometer needle will be in balanced position, permitting chopper bar 333 to close mercury switch H8 and moving step switch 91 from control point I to control point 2, thereby disconnecting the galvanometer from slide wire 88 and connecting it to slide wire 88 simultaneously extinguishing light 1 and lighting the bulb for control point 2, deenergizing the solenoid of valve 53 and energizing the solenoid of valve ltd thereby connecting controlled air pressure through valve 144 to the controller l3! and resetting the control point thereof for reflux rate #2. Bulb 853 will be extinguished and the bulb for reflux rate #2 will be lighted. No change will be made in the product valves or the slop valves.

When the set point on slide wire 80 is reached, the step switch 91 is moved to control point #3, connecting slide wire 80 to the Wheatstone bridge and disconnecting slide 802 therefrom, simultaneously lighting bulb 3 and extinguishing bulb 2, resetting controller [3? for reflux rate #3, extinguishing the bulb for reflux rate #2 and lighting the bulb for reflux rate #3. No change is made in the product valves or the slop valves.

When the set point on slide wire is reached, the galvanometer is disconnected from slide wire 38 and is connected to the holding coils 92 and so, thereby holding the galvanometer needle on the low setting, step switch 91 is moved to control point l, control point bulb 3 is extinguished and bulb 4 is lighted, reflux rate is changed from rate #3 to #1, reflux rate #3 light is extinguished and #1 light is lighted, time delay TD-2 is energized which holds product valve ldl open for a predetermined period of time to clear pipe 25, pump 2i, pipe 28, cooler 2% and pipe to which clears the product lines up to the product valve manifold of product 1. At the expiration of the set time period, TD? energizes the coil of relay R--? which looks up mechanically and opens one side of the power line to the product valve solenoids thereby venting air from the diaphragm of product valve lfii and closing this valve at the same time extinguishing light 164. Simultaneously time delay mechanism TD-3 is energized, thereby energizing the solenoid of valve 599, admitting air to the diaphragm of slop valve 48 and opening this valve. At the same time bulb 482 is lit. At the expiration of the set time of TD--3, the solenoid of valve I99 is deenergized, the valve is closed, and bulb 92 is extinguished, release coil i of relay Psl is energized thereby opening relay Rr-T, the coil of relay R-B is energized, closing this relay, and connecting the galvanometer to coils 9i! and 9| in addition to the coils 92 and 93, causing the step switch ill to move the step switch to point 4, deenergizing TD-2 and TD-3 thereby allowing these timers to reset and to restore power to lead 233 thus permitting the proper product valve to open, simultaneously connecting slide Wire 89 in the Wheatstone bridge, opening the valve controlling product #2, lighting the bulb for product #2, also energizing the release coil of relay R| and opening this relay, deenergizing the coil of solenoid 2.29 which results in the closing of valve 268 in vapor line 299, extinguishing bulb 324, simultaneously energizing the coil of solenoid 315, permitting air from the diaphragm of valve 2% to escape through valve 203 to the atmosphere, opening valve 2% and lighting bulb SIT.

The operation of the control system at control point l is like the operation at control point 1. The operation at point 5 is like point 2, the operation at point 6 is like the operation at point 3, and the operation at point 7' is like the operation at point i.

The operation at control point 7 is the same as the operation at control point 1 excepting that relay R-% is energized and is locked up mechanically, which results in the energization of sole noid 3&9 controlling valve 231 in the air line to which pressure indicator controller 53 is connected, thereby moving valve 23! and resetting controller 53 from the control point set for ten pounds to the control point set for one-half pound gage, at the same time lighting bulb 3i I. It will be understood that this operation occurs only at control point '7.

Thereafter the operations previously described are repeatedin their proper order until the end of the batch distillation run.

When the temperature in the distillation unit rises to the point set on slide wire '80, "step switch 97 will move as previously described irom control point 24 to control point 25' which disconnects the galvanometer from slide wire 80 and connects galvanoine'ter T4 to the holding coils 92 and 93 thereby "preventing the step switch from moving further. Simultaneously the light 24 is extinguished, the solenoid of valve I48 controlling reflux rate #3 is deenergized, extinguishing the bulb for reflux rate #3, and the solenoid of 'valve I34 is energized, bulb 1 53 --for reflux rate #1, and changing the control point setting of the controller I31 to change the reflux rate from the #3 rate to the 1 rate. Also simultaneously PD-2 is energized and at the end of the time delay period, relay Rl is energized and locks up mechanically and disconnects the power line :r-m'n the product valves, closing the product valve in line '38 and extinguishing product #Blieht, energizing timer FED-3, opening slop valve 48 and lighting bulb I92. At the end of the time delay :pe'riod, slop valve 38 is closed and bulb J92 extinguished, the release coil of relay R l is 'enetgized, causing this relay to release and open, and simultaneously the coil of relay lit-B is energized, connecting the galvanometer also to the coils 9'0 and 9!, causing step switch 91 to move rmm control point 25 to point which @again connects the galvanometer to the holding coils 92 and 93, lighting bulb TE, energizing the "release coils of relays R-l and-R d opening these relays and deenergizing the motor starting equipment 244 thereby stopping the product pump 2 then in operation, simultaneously deeriergizing' 'solenoid 256 thereby closing valve 25'5'in air line 253 which controls valve 251 in steam line 14 closing valve 25!, extinguishing bill!) 259 and shutting off the supply of steam to the .coil relay RP-S, allowing this relay to open, also simultaneously deenergizing the coil of solenoid valve I34, controlling reflux rate #1, extinguishing bulb I53, closing the flowcontrol valve 139 in product line 30, simultaneously energizing the relay RI which locks up mechanically and deenergizes the solenoid 3-1 5, causing valve 205 "to close, extinguishing bulb 8 -11, energizing the solenoid 32l, opening valve 208, lighting bulb 324, also simultaneously energizing release coil of relay R-'8, thereby opening the relay, deenergizing solenoid 3:09, .perrni-tting controller 163 to reset from one half p'oun'd control to ten pounds control, extinguishing bulb '31! and simultaneously connecting :push button 125 'to the power line. 'At this :point the control system has completed its operation for the batch distillation run.

In the event of high still pressure, the release coils of relays Rw-i and It- 2 will be energized and shut down the unit by shutting off the steam and shutting down the product pump. The howler 6| is simultaneously sounded and light 283 lit until the still pressure drops below the set point of controller .62. To start up the unit again reset button 188 must b'e rnov'ed to closed position to reenergize-'1*elay-lR-=4,after which push button 229 is moved to'closed position to reenergize relay and to put the -distillation unit back in operation automatic control.

In the event of low steam ipr'es'sure, mercury switch 263 is closed a'nd swath =21! is opened. The first o "sultsih the sounding'of howler fil gliting 239,' tl fe l3, also deenergizing second operation resulting in the deenergization of most of the control system including coil 256 and the motor starter coils, shutting down the unit excepting that relays R-4 and RF-5 are not released so that the unit will start up again automatically on the restoration of normal steam pressure. Power failure has the same efiect on the unit and also deenergizes solenoid 293 admitting air to whistle 291' causing the same to sound. Air failure closes the steam and product valves due to the release .of the air pressure controlling these valves, inasmuch as all of these valves are of the type that are opened under air pressure and'are closed when the pressure is released. Air failure also allows mercury switch 284 to close energizing relay 288 causing the hoWler 6| to sound and bulb 290 to light.

Any power interruption will deenergize solenoid 3l5 and open valve 205. This valve is also opened upon air failure.

Continuous batch distillation may be carried out with the apparatus disclosed hereinbefore, by charging the still through line H, Fig. l, :by pump 12, and by employing a control device'4l5 which is responsive to the level of liquid the still to control a valve .418 in the feed line. 0ontinuous batch distillation operation is particularly applicable in cases where a substantial.

portion of the charge to the distillation unit, consisting of the lighter boiling constituents, may be removed as a single fraction. The charge is fed to the still Ill at a rate such that the first light out is fed to the -still"at a rate substantially equal to the rate at which it is removed from the still by fractional distillation. The desired charge rate is controlled and maintained by flow recorder controller Ml which controls the setting of control valve 420. The still 'is heated at the desired rate substantially constantly during the entiredistillation period. This operation is the equivalent of a continuous shell still operation in which the residue is accumulated in the still and this accumulation continues until the liquid in the still reaches a predetermined level, at which the controller 415 closes valve M6 and cuts off the supply of feed to the still. After the feed is cut oil, the distillation continues as a discontinuous batch operation in the manner described shereinbefore in connection with the batch distillation operation. The temperature at the top of the tower "gradually rises, and the level of the temperature of the vapors at the top is-employedas a basis for the automatic control of the distillation operation, regulating the reflux ratios by predetermined steps :and controlling the product line valves so as to produce the desired products in the desired degrees of purity, all in the manner 'he-r-einbeiore disclosed. The same automatic safetydevices as previous"- ly disclosed are employed, and the heating-steam is automaticallyshut oil and the "unit shut down automatically at the end of the run as previously described. 1

In lieu of changing the reflux ratio when "certain predetermined temperatures are reached, as previously described, the reflux to the column may be regulated automatically and continuously in response to the temperature at the base of the column so as to produce an overhead-product of' the desired purity, while using at all times the minimum permissiblereflux ratio. By so controlling the reflux,:a'specified-overhead prodnot can be produced with the absolute minimum amount' of flieatcorisu med inboiling' theiiqu idin the still. This method or operation is' iaaiiticularly applicable to the close fractionation of a two-component mixture. An equation can be determined which will indicate the reflux ratio required to produce an overhead product of any specified purity, expressed in terms of the composition of the vapor entering the base of the fractionation column as feed. This composition, in the case of a two-component mixture, can be expressed readily in terms of temperature, in consequence of which it is possible to calculate an equation expressing reflux ratio required as a function of the temperature at the base of the tower. Operating in accordance therewith, a thermometer resistance bulb fill is located at the bottom portion of the tower, and is connected through suitable mechanism in the control system to the controller I3! for reflux control valve I39, the mechanism being operative to provide that reflux ratio which will produce the overhead product desired with the minimum permissible reflux ratio. One form of such mechanism would be similar to the pressure-temperature compensator hereinbefore described, containing a cam of suitable shape which in this case would be operated in response to variations in temperature of thermometer resistance bulb 4Ii functioning so as to reset the control mechanism of flow recorder controller I31. A second thermometer resistance bulb, like bulb 55, will be utilized to shut down the unit automatically as soon as all of the lighter constituent of the desired purity has been removed from the still. When this point has been reached, and the maximum reflux ratios are being used, the temperature will begin to rise above a point which will correspond to overhead product of acceptable purity, and the control system will operate automatically and immediately to shut down the unit, the end of the run having been reached. This method of operation may be employed either with a distillation unit in which the still is charged completely before the heat is turned on as previously described in connection with the discontinuous batch distillation method, or it can be used with a continuous batch unit as described previously, in which the charge is slowly pumped into the still while the still is being heated at a predetermined rate. This method of operation also may be applied to multiple component distillation by providing a suitable mechanical and electrical mechanism for the resetting of flow recorder controller 531 for each individual product, these mechanisms being connected at the proper stage of the distillation in substantially the same manner as the several slide wires previously described.

In another method of automatic continuous batch distillation, the rate of charging of the still is controlled by a flow recorder controller which is reset as necessary so as to maintain a constant temperature of the liquid within the still up to the time that the charge of the still is terminated as a result of the level in the still having reached a predetermined point. The operation of the unit will be substantially as follows: Starting with an empty still, the steam will be admitted into the heating coil I3 (Fig. 1) through the steam line It, the rate of admission of the steam being controlled by a control valve 25I in response to the action of a flow recorder controller M9 similar to controller 59 with the addition of a mechanism responsive to the temperature of thermometer resistance bulb 422 located in the still which operates to reset the con trol setting of flow recorder controller 42L The charge to the still will be pumped into the unit through feed line H by feed pump I2, the rate of flow being controlled by a valve 425, the opening of which is controlled by a flow recorder controller 42I similar to controller 59. As the charge to the still is heated, a portion of it is vaporized, the vapors passing into column I9 and flowing counter-current to and in contact with reflux, and a portion of the condensate of the overhead vapors is withdrawn through line 2% and pumped by pump 21 through line 28 and cooler 29 to product line 30. The balance of the condensate of the overhead vapors, after passing downwardly through the column I9, returns to the still Ill through reflux return line 40. A thermometer esistance bulb G22 which is immersed in the liquid within the still I0, is connected through the control system by suitable mechanical and electrical means similar to that previously disclosed, to the flow recorder controller MI in such manner as to control the rate of admission of feed to the still by control valve 420 to maintain a substantially constant temperature within the still. The control system will be set so that the temperature within the still is maintained at a point corresponding to partial vaporization of the feed. In consequence, the level of the liquid within the still will increase continually until eventually the level therein reaches a predetermined point, at which the liquid level controller M5 will operate to close valve Mil in feed line II and terminate the flow of feed into the still. As soon as the flow of feed into the still is cut off, the temperature of the liquid in the still will begin to rise and it will no longer be possible for the flow recorder controller 42I to control the temperature of the liquid within the still. As the temperature of the liquid in the still rises, the composition of the vapors leaving the still will change, becom ing more concentrated in heavier constituents than previously. Up to this time the relationship between the quantity of reflux liquid withdrawn through line 26 as product and the reflux liquid returned through the column will have been controlled by flow recorder controller I31 operating through valve I39, so that the composition of the product will have remained substantially constant, and the temperature of the vapors leaving the top of the column, as indicated by thermometer resistance bulb 55, will have remained substantially constant.

As soon as the temperature of the vapors entering the base of column l9 begins to rise. the temperature at the top of the column also will tend to rise. As the temperature at the top of the column reaches predetermined temperature levels, the control system will operate so as to reset flow recorder I3'l thereby changing the setting of control valve I39 and, by decreasing the rate of flow of product through line 30, will increase the reflux ratio within the fractionating column, thereby tending to prevent the temperature at the top of the column from increasing.

When the temperature at the top of the column reaches a predetermined temperature which corresponds to the exhaustion of the lightest boiling constituent from the still feed, the control system will operate to close control valve It! in product line 3|, simultaneously opening control valve I6I in product line 32, thereby terminating the flow of product #1 from the column and beginning the flow of product #2 through line 32. The distillation then continues with the temperature at the top of the column rising and with the control system having reset new recorder controller I31, thereby changing the position of valve I39 to permit an increase in the rate of flow of product through line 30, valve I6! and line 322 to the tank collecting product #2. As the temperature continues to rise, the control system, at fixed temperature points, resets the flow controller I31 and changes the setting of the valve '39, thereby altering the reflux ratio within the column and tending to prevent a rise in the temperature at the top of the column. This will continue in the manner previously described, until a final temperature is reached at the top of the column, at which point the control system will close valve l6! and open valve 55 in product line 33, thereby terminating the flow of product #2 and initiating flow of product #3. It will be understood that as many products as desired may be produced by a continuation of this procedure.

In accordance with another method of control, a third thermometer resistance bulb 126, Fig, l, is placed in the vapor stream leaving the top of the column, which will operate to reset flow recorder controller I31 thereby varying the rate of flow of product from the unit and continuously controlling the reflux ratio within the unit, increas ng the reflux ratio as the temperature in the top of the column tends to rise until a maximum allowable reflux ratio is attained. After the maximum allowable reflux ratio i attained, the temperature of the vapors leaving the top of the column will rise and thermometer resistance bulb 55, Fig. 2, will operate as described previously to open slop valve '48 and complete the operating cycle in the case of two-component distillation, or to connect in a new slide Wire and continue the distillation operation in the case of multiple component distillation.

A further method of control utilizes thermometer resistance bulb 55 as the means of resetting flow recorder controller I31 and controlling the reflux ratio within the fractlonating column, causing the reflux ratio to increase substantially continuously as the distillation of a particular component progresses until a predetermined maximum reflux ratio is obtained, at which time the control mechanism operates to terminate the distillation as described previously in the case of a single component distillation, or to terminate the production of one product and connect in another slide wire for the production of another product in the case of multiple-component distillation.

Use of the apparatus and the methods of control herein disclosed, make possible the production of products more closely fractionated than has been possible heretofore in the art on a commercial scale, and also makes possible the production of products of normal degree of purity, with a lower consumption of heat and other utilities than has been possible hitherto.

The present application is a continuation of application Serial'No. 389,756 filed April 22, 1941, and which is now abandoned.

Inasmuch as changes may be made in the form,-

location and relative arrangement of the several parts of the apparatus disclosed, and changes maybe made in the several steps of the methods disclosed and in their sequence, and certain parts of the apparatus disclosed and certain method steps disclosed may be omitted, if desired, without materially altering the function or operation of the parts of steps remaining, it will be understood that the invention is not to be limited excepting by the scope of the appended claims.

What is claimed is:

1. Apparatus for the batch distillation of composite liquid comprising a still, a fractionating column, means for supplying heat to the still, means for introducing into the lower part of the column liquid vaporized in the still, means in the column for passing vapors or the liquid countercurrent to and in contact with reflux, means for condensing substantially all of the overhead vapors and returningipart of the condensate to the column as reflux, a conduit through which product distillate is withdrawn from the column, a valve in said conduit for controlling the rate at which product distillate is withdrawn from the column thereby controlling the reflux rate, tem perature responsive means in the path of flow of the overhead vapors, control means actuated by the temperature responsive means to control the valve in the conduit during the production of a distillate fraction, said control means being operative in response to said temperature responsive means to maintain the withdrawal rate of the product distillate constant at each of successively difierent increasing values between said temperature limits and, until production of the fraction is completed, to decrease the withdrawal rate of the product distillate abruptly from a higher to a succeeding lower value when predetermined distillate vapor temperatures are successively reached, and pressure responsive means to the pressure of the distillate vapors for compensating the response of the temperature actuated control means for deviations of the pressure of the distillate vapors from a predetermined pressure.

2. Apparatus for the batch distillation of composite liquid comprising a still, a fractionating column, means for supplying heat to the still, means for introducing into the lower part of the column liquid vaporized in the still, means in the column for passing vapors of the liquid counter-current to and in contact with reflux, means for condensing substantially all of the overhead vapors and returning part of the condensate to the column as reflux, a conduit through which product distillate is withdrawn from the column, a valve in said conduit for controlling the rate at which product distillate is withdrawn from the column thereby controlling the reflux rate, temperature responsive means in the path of the overhead vapors, control means actuated by the temperature responsive means to control the valve in the conduit during the production of a distillate fraction, said control means being operative in response to said temperature responsive means to maintain the reflux ratio constant at each of successively diiferent increasing values between said temperature limits and, until production of the fraction is completed, to increase the reflux ratio abruptly from a lower to a higher succeeding value when predetermined distillate vapor temperatures are successively reached, and pressure responsive means responsive to the pressure of the distillate vapors for compensating the response of the temperature actuated control means fordeviations of the pressure of the distillate vapors from a predetermined pressure.

3. Apparatus for the batch distillation of com posite liquid comprising a still, a fractionating column, means for supplying heat to the still, means for introducing into the lower part of the column liquid vaporized in the still, means in the column for passing vaporsof the liquid countercurrent to and in contact with reflux, means for condensing substantially all of the overhead vapors and returning part of the condensate to the column as reflux, a conduit through which product distillate is withdrawn from the columnv a valve in said conduit for controlling the rate at which product distillate is withdrawn from the column thereby controlling the reflux rate, temperature responsive means in the path of the overhead vapors, control means actuated by the temperature responsive means to control the valve in the conduit during the production of a distillate fraction, said control means being operative in response to said temperature responsive means to maintain the withdrawal rate of the product distillate constant and to maintain the reflux ratio constant at each of successively different values between said temperature limits and, until production of the fraction is completed, to increase the reflux ratio abruptly from a lower to a higher successive value and to decrease the withdrawal rate of the product distillate abruptly from a higher to a lower successive value when predetermined temperatures are successively reached, and pressure responsive means responsive to the pressure of the distillate vapors for compensating the response of the temperature actuated control means for deviations of the pressure of the distillate vapors from a predetermined pressure.

4. Apparatus for the batch distillation of composite liquid comprising a still, a fractionating column, means for supplying heat to the still, means for introducing into the lower part of the column liquid vaporized in the still, means in the column for passing vapors of the liquid counter-current to'and in contact with reflux, means for condensing substantially all of the overhead vapors and returning part of the condensate to the column as reflux, a conduit through which product distillate is withdrawn from the column, a valve in said conduit for controlling the rate at which product distillate is withdrawn from the column thereby controlling the reflux rate, a plurality of product lines connecting with said conduit and each having a valve therein, temperature responsive means in the path of the overhead vapors, control means actuated by the temperature responsive means to control the valve in the conduit during the production of a distillate fraction, said control means being operative in response to the temperature responsive means to maintain the reflux ratio constant at each of successively different increasing values between said temperature limits and, until production of the fraction is completed, to increase the reflux ratio abruptly from a lower to a higher successive value when predetermined tempera.- tures are successively reached and other means operative in response to said control means for successively opening the valves in the product lines one at a time and closing the open valve prior to opening another valve in the product lines.

5. Apparatus for the batch distillation of composite liquid comprising a still, a fractionating column, means for supplying heat to the still, means for introducing into the lower part of the column liquid vaporized in the still, means in the column for passing vapors of the liquid counter-current to and in contact with reflux, means for condensing overhead vapors and returning condensate to the column as reflux, a conduit through which product distillate is withdrawn from the column, a valve in said conduit for controlling the rate at which product distillate is withdrawn from the column thereb controlling the reflux rate, a thermometer resistance bulb in the path of said overhead vapors, a Wheatstone bridge including a galvanometcr, said bulb being connected between fixed resistances in one side of the Wheatstone bridge, a plurality of slide wires of different resistances and each having a slider in contact therewith, first electrical switch means for selectively connecting the slide wires into the Wheatstone bridge between fixed resistances in the other side of the bridge and disconnecting them therefrom, one side of the galvanometer being connected to said bulb and the other side being connected to the sliders of said slide wires, and second electrical switch means operative simultaneously with the first switch means for reg-- ulating the setting of the valve in said conduit thereby to control the reflux rate.

6. Apparatus for the batch distillation of com-- posite liquids comprising a still, a fractionating column, means for supplying heat to the still. means for introducing into the lower part of the column liquid vaporized in the still, means in the column for passing vapors of the liquid counter-current to and in contact with reflux, means for condensing substantially all of the overhead vapors and returning part of the condensate to the column as reflux, a conduit through which product distillate is withdrawn from the column, a valve in said conduit for controlling the rate at which product distillate is withdrawn from the column thereby controlling the reflux rate, a plurality of product lines connecting with said conduit and each having a valve therein, a temperature measuring device in the path of said overhead vapors, means operative in response to said device for regulating the setting of the valve in said conduit thereby to control the reflux rate, other means operative in response to said device for controlling the valves in said product lines, a second temperature measuring device in the path of said overhead vapors, and means operative in response to said last mentioned device for compensating the raspouse of the first mentioned device for deviations of the pressure of the overhead vapors from a predetermined pressure.

'7. Apparatus for the batch distillation of composite liquids comprising a still, a fractionating column, means for supplying heat to the still, means for introducing into the lower part of the column liquid vaporized in the still, means in the column for passing vapors of the liquid counter-current to and in contact with reflux, means for condensing overhead vapors and returning condensate to the coluunn as reflux, a conduit through which product distillate is withdrawn from the column, a valve in said conduit for controlling the rate at which product dist-illate is withdrawn from the column thereby controlling the reflux rate, a plurality of product lines connecting with said conduit and each having a valve therein, a thermometer resistance bulb in the path of said overhead vapors, a Wheatstone bridge including a galvanometer, said bulb being connected between fixed resistances in one side of the Wheatstone bridge, a plurality of slide wires of difierent resistances and each having a slider in contact therewith. first electrical switch means for selectively connecting the slide wires into the Wheatstonc bridge between fixed resistances in the other side of the bridge and disconnecting them thereaszazso from, one side of the galvanometer being connected to said bulb and the other side being connected to the sliders of said slide wires, secand electrical switch means operative simultaneously with the first switch means for regulating the setting of the valve in said conduit thereby to control the reflux rate, and third electrical switch means operative simultaneously with said other switch means for controlling the valves in said product lines.

8. Apparatus for the batch distillation of composite liquids comprising a still, a fractionating column, means for supplying heat to the still, means for introducing into the lower part of the column liquid vaporized in the still, means in the column for passing vapors of the liquid counter-current to and in contact with reflux, means for condensing overhead vapors and re" turning condensate to the column as reflux, a conduit through which product distillate is withdrawn from the column, a valve in said conduit for controlling the rate at which product distillate is withdrawn from the column thereby controlling the reflux rate, a plurality of product lines connecting with said conduit and each having a valve therein, a thermometer resistance bulb in the path of said overhead vapors, a Wheatstone bridge including a galvanometer, said bulb being connected between fixed resist= ances in one side of the Wheatstone bridge, a plurality of slide wires of diflerent resistances and each having a slider in contact therewith, first electrical switch means for selectively connecting the slide wires into the Wheatstone bridge between fixed resistances in the other side of the bridge and disconnecting them therefrom, means for compensating the temperature measurement for variations of pressure in the column comprising another slide wire connected to said bulb and between said fixed resistances in said one side of the Wheatstone bridge, a slider movable in contact with said other slide wire and connected to one side of the galvanometer, the other side of the galvanometer being connected to the sliders of the first mentioned slide wires, a second thermometer resistance bulb connected in parallel with said other slide wire, a member comprising a movable pneumatic nozzle, another member comprising a flapper arranged to oppose the escape of air from the nozzle and movable with respect thereto, means for moving one member in response to variations in pressure in the column, a cam, means for moving the cam in response to variations in the relative positions of the nozzle and the flapper, the movement of the other member being controlled by the movement and contour of the cam, means for moving the slider associated with said other slide wire with the cam, second electrical switch means operative simultaneously with the first switch means for regulating the setting of the valve in said conduit thereby to control the reflux rate, and third electrical switch means operative simultaneously with said other switch means for controlling the valves in said product lines.

9. Apparatus for the batch distillation of composite liquids comprising a still, a fractionating column, means for supplying heat to the still, means for introducing into the lower part of the column liquid vaporized in the still, means in the column for passing vapors of the liquid countercurrent to and in contact with reflux, means for condensing overhead vapors and returning condensate to the column as reflux, a conduit through which product distillate is withdrawn from the 30 column, a valve in said conduit for controlling the rate at which product distillate is withdrawn from the column thereby controlling the reflux rate, a plurality of product lines connectingwith said conduit and each having a valve therein, a plurality of slop lines connecting with said conduit and each having a slop valve therein, a thermometer resistance bulb in the path of said overhead vapors, a Wheatstone bridge including a galvanometer, said bulb being connected between fixedresistances in one side of the Wheatstone bridge, a plurality of slide wires of difierent resistances and each having a slider in contact therewith, first electrical switch means for selectively connecting the slide wires into the Wheatstone bridge between fixed resistances in the other side of the bridge and disconnecting them therefrom, means for compensating the temperature measurement for variations of pressure in the columncomprising another slide wire connected to said bulb and between said fixed resistances in said one side of the Wheatstone bridge, a slider movable in contact with said other slide wire and connected to one side of the galvanometer, the other side of the galvanometer being connected to the sliders of the first mentioned slide wires, a second thermometer resistance bulb connected in parallel with said other slide wire, a member comprising a, movable pneumatic nozzle, another member comprising a flapper arranged to oppose the escape of air from the nozzle and movable with respect thereto, means for moving one member in response to variations in pressure in the column, a cam, means for moving the cam in response to variations in the relative positions of the nozzle and the flapper, the movement of the other member being controlled by the movement and contour of the cam, means for moving the slider associated with said other slide wire with the cam, second electrical switch means operative simultaneously with the first switch means for regulating the setting of the valve in said conduit thereby to control the reflux rate, third electrical switch means operative simultaneously with said other switch means for controlling the valves in said product lines, fourth electrical switch means operative simultaneously with said other switch means for controlling said slop valves, relay means electrically associated with certain of said switch means, and time delay mechanisms, associated with the switch means controlling the product valves and slop valves.

10. Apparatus for the batch distillation of composite liquids comprising a still, a fractionating column, means for supplying heat to the still, means for introducing into the lower part of the column liquid vaporized in the still, means in the column for passing vapors of the liquid countercurrent to and in contact with reflux, means for condensing overhead vapors and returning condensate to the column as reflux, a conduit through which product distillate is withdrawn from the column, a valve in said conduit for controlling the rate at which product distillate is withdrawn from the column thereby controlling the reflux rate, a plurality of product lines connecting with said conduit and each having a valve therein, a plurality of slop lines connecting with said conduit and each having a slop valve therein, a thermometer resistance bulb in the path of said overhead vapors, a Wheatstone bridge including a galvanometer, said bulb being connected between fixed resistances in one side of the Wheatstone bridge, a plurality of slide wires of difierent re- 

